O modelamento estatístico de misturas: experimento tutorial usando voltametria de redissolução anódica

This work illustrates the modeling procedure for a solvent mixture using the simplex- centroid approach. The selected experiment was the optimization of the peak current observed in the direct determination of nickel by anodic stripping voltammetry (ASV) in a solvent mixture composed of N,N-dimethylformamide, ethanol and water. The text is presented in a tutorial way, showing in detail the several steps which must be followed in such a process. Since not all possible mixtures lead to a measurable instrumental response, pseudocomponents had to be used to rescale the experimental design. This also allows to show how to apply this tool, usually troublesome for non-specialists in mixture modeling procedures.

Desenvolvimento e validação de metodologia de análise de misturas biodiesel: diesel utilizando cromatografia gasosa-espectrometria de massas

The aim of this work was to develop and validate a method of analysis of biodiesel:diesel blends using HRGC-MS in SIM mode. The proposed method is applicable to biodiesel from linoleic oils, such as soybean oil. The following results were obtained: linearity over the methyl linoleate concentration range of 250-2500 mg L-1 (R² > 0.999); limits of detection and quantification of 2 and 5 mg L-1, respectively; recovery from 82 to 96% of biodiesel in diesel and repeatability < 2% (RSD). Comparison between two operators showed that it is not necessary the same operator to do the analysis.

Determinação de misturas de sulfametoxazol e trimetoprima por espectroscopia eletrônica multivariada

In this work a multivariate spectroscopic methodology is proposed for quantitative determination of sulfamethoxazole and trimethoprim in pharmaceutical associations. The multivariate model was developed by partial least-squares regression, using twenty synthetic mixtures and the spectral region between 190 and 350 nm. In the validation stage, which involved the analysis of five synthetic mixtures, prediction errors lower that 3% were observed. The predictive capacity of the multivariate models is seriously affected by spectral changes induced by pH variations, a fact that acquires a great significance in the analysis of real samples (pharmaceuticals) that contain chemical additives.

Aplicação de zeólitas sintéticas como coadjuvante em formulação detergente

The study consists is the application of zeolites NaX, NaY and A as builder in detergent formulations to eliminate the hardness of water. Therefore, the adsorption of ions Ca+2 and Mg+2 were evaluated, and the effect of the cleaning action of the surfactant sodium dodecil sulfate (SDS) through tests of detergency. The experiments were conducted in bath system (with shaking) and quantification of metals was performed by atomic absorption spectrometry. Zeolite A showed the best results for adsorption of Ca++ and Mg++ with retention rates of around 90 and 70% respectively and acted positively on the action of cleaning the surfactant SDS.

Adsorção e propriedades de volume de misturas binárias água álcool: um experimento didático com base em medidas de tensão superficial

An undergraduate physical chemistry experiment based on the drop counting method for surface tension measurements is proposed to demonstrate adsorption isotherms of binary aqueous solutions of ethanol, n-propanol, and n-butanol. Excess surface is obtained by the derivative of surface tension taken with respect to alcohol activity, after this activity calculation using van Laar equation. Laboratory class contents are surface tension, excess surface, percolation of hydrogen bonds, micelle, activity, and ideal solution.

Autoassociação de misturas dos Surfactantes Dodecanoato de Sódio (SDoD) e Decanoato de Sódio (SDeC) com o Polímero Hidrofobicamente Modificado Etil(Hidroxietil)Celulose (EHEC)

In this work, the interactions between the non-ionic polymer of ethyl(hydroxyethyl)cellulose (EHEC) and mixed anionic surfactant sodium dodecanoate (SDoD)-sodium decanoate (SDeC) in aqueous media, at pH 9.2 (20 mM borate/NaOH buffer) were investigated by electric conductivity and light transmittance measurements at 25 ºC. The parameters of the surfactant to polymer association processes such as the critical aggregation concentration and saturation of the polymer by surfactants were determined from plots of specific conductivity vs total surfactant concentration, [surfactant]tot = [SDoD] + [SDeC]. Through the results was not observed a specific link of polymer with the surfactant, implying therefore a phenomenon only cooperative association.

Uso da cromatografia gasosa bidimensional abrangente (GC×GC) na caracterização de misturas biodiesel/diesel: aplicação ao biodiesel de sebo bovino

The growth of biodiesel market and the implementation of regulations related to biodiesel production and biodiesel/diesel blending has encouraged the development of appropriate analytical methods to control the composition of this type of mixture. In this study, an evaluation of the potential of GC×GC for the characterization of samples of beef tallow biodiesel and the composition of blends of biodiesel/diesel is presented. The methodology was applied to beef tallow biodiesel and its mixtures with petrodiesel, ranging from B2 to B50. Results allowed not only the identification and quantification of the biodiesel esters, but also the biodiesel percentage in biodiesel/diesel blends.

Uso de redes neurais recorrentes na determinação das constantes de acidez para a 7-epiclusianona em misturas etanol-água

This work propose a recursive neural network to solve inverse equilibrium problem. The acidity constants of 7-epiclusianone in ethanol-water binary mixtures were determined from multiwavelength spectrophotmetric data. A linear relationship between acidity constants and the %w/v of ethanol in the solvent mixture was observed. The proposed method efficiency is compared with the Simplex method, commonly used in nonlinear optimization techniques. The neural network method is simple, numerically stable and has a broad range of applicability.

Modelos ridge em planejamentos de misturas: uma aplicação na extração da polpa de pequi

Mixture Models can be used in experimental situations involving areas related to food science and chemistry. Some problems of a statistical nature can be found, such as effects of multicollinearity that result in uncertainty in the optimization of a dependent variable. This study proposes the application of the ridge model adapted for mixture planning considering the Kronecker (K-model) and Scheffe (S-Model) methods applied to response surfaces. The method determined the proportions of hexane, acetone and alcohol proportions that resulted in the maximum response of percentage of extracted pequi (Caryocar brasiliense) pulp oil.

Efeito da ativação mecânica de uma formulação de talco/caulim/alumina sobre o mecanismo e a cinética de formação de cordierita

In this study, the influence of mechanical activation by intensive ball milling of a stoichiometric mixture of talc, kaolin, and alumina on the mechanism and kinetics of cordierite (2MgO·2Al2O3·5SiO2) formation was evaluated. The raw materials were characterized by chemical analysis, X-ray diffraction (XRD), laser diffraction, and helium pycnometry. The kinetics and mechanism of cordierite formation were studied by XRD, differential thermal analysis, and dilatometry in order to describe the phase formation as a function of temperature (1000-1400 ºC), time of thermochemical treatment (0-4 h), and grinding time of the mixture (0-45 min). Finally, the optimal conditions of the thermochemical treatment that ensured the formation of cordierite were determined: milling time of 45 min and thermal treatment at 1280 ºC for 1 h.

Otimização da etapa de extração do ácido clavulânico presente no caldo de fermentação utilizando misturas de solventes

The purpose of this work was to study four different solvent mixtures intended to increase the yield of the extraction stage of clavulanic acid (CA), which is one of the steps in the purification process. Four central composite rotatable designs (CCRD) were utilized to optimize the solvent mixtures. The variables selected for the factorial design were solvent mixture ratio (mL/mL) and temperature (ºC). The results showed that the yield of CA extracted from fermentation broth with the solvent mixtures of methyl-ethyl-ketone and ethyl acetate, and methyl-isobutyl-ketone and ethyl acetate (44.7 and 50.0%, respectively) was higher than that of the individual ethyl acetate alone (36.5%).

DESENVOLVIMENTO DE ENSAIO PARA ANÁLISE QUALITATIVA DE BIODIESEL EM MISTURAS DIESEL-BIODIESEL PARA APLICAÇÃO EM POSTOS REVENDEDORES DE COMBUSTÍVEIS

In this study, we developed a method for the visual detection of biodiesel in petrodiesel-biodiesel (BX) blends through the aminolysis of the methyl or ethyl esters of fatty acids that are found in biodiesel and that are absent from diesel and vegetable oils. This method is based on three reactional stages, which produce a dark red and easily visualized complex in the presence of biodiesel. In the absence of biodiesel, there is no dark red coloring, whereas in the presence of diesel or vegetable oil, there is a light red to yellow coloring. This simple, practical, inexpensive, and effective procedure may be applied by petrol stations to guarantee to consumers and resellers the presence of biodiesel in diesel blends, regardless of the BX blend's initial coloring or of the sulfur found in the diesel. In short, it ensures a safe fuel tank fill-up with BX blend.

Desenvolvimento de metodologia simplificada para análise de hexametilenotetramina (hmt) em medicamentos contendo corantes em sua formulação

No presente trabalho desenvolveu-se metodologia simplificada para análise de hexametilenotetramina em medicamentos que apresentam corantes em sua formulação (azul de metileno, Ponceau Red, Bordeaux Red, acriflavina) seguida por titulação ácido-base usando indicador. O método foi aplicado com sucesso a amostras comerciais e os resultados obtidos foram comparados com aqueles encontrados por titulação potenciométrica, apresentando muito boa concordância. Recobrimentos situaram-se na faixa de 101,3 - 104,2%, com desvios padrão de 0,1 - 2,1.

Estudo de estabilidade do fosfato dissódico de prednisolona em condições de estresse oxidativo e térmico, em formulação oral

Este trabalho consistiu em investigar o processo de degradação do fármaco Fosfato Sódico de Prednisolona (FSP) na forma farmacêutica de solução oral por meio de ensaios de degradação, avaliando-se os parâmetros de acordo com a Resolução nº. 899/2003 da ANVISA e o processo de degradação do fármaco. O método por cromatografia líquida de alta eficiência (CLAE), desenvolvido para o doseamento do fármaco, foi validado a fim de comprovar sua aplicabilidade como indicativo de estabilidade, assegurando a confiabilidade do mesmo. Após o método ser validado no estudo da degradação do fármaco, comprovou-se que em condições drásticas de estresse oxidativo (H2O2 30%) e temperatura a 60°C, a degradação do fármaco é dependente de sua concentração (cinética de primeira ordem). Os resultados apresentaram-se satisfatórios, demonstrando que este método é adequado para investigação da formação de produtos de degradação na forma farmacêutica solução oral.

Eficiência de nova formulação do herbicida oxyfluorfen no controle de plantas daninhas em área de Pinus caribea Morelet var. hondurensis Barr. et Golf

Foi realizado um experimento para avaliar a seletividade e a eficiência do herbicida oxyfluorfen5 formulado a 480 e 240 g/l, em área com mudas de Pinus caribea Morelet var. hondurensis Barr. et Golf. recém-transplantadas (aplicação em pré-emergência das plantas daninhas) e com 12 dias após o transplante (aplicação em pós-emergência inicial das plantas daninhas). O ensaio foi instalado no município de Paulínia, Estado de São Paulo, em um Latossolo Vermelho-Escuro, eutrófico, no ano agrícola 1999/2000. Foi adotado o delineamento em parcelas subsubdivididas no tempo, tendo como tratamento principal, disposto em blocos ao acaso com quatro repetições, o herbicida oxyfluorfen formulado a 480 g/l de ingrediente ativo (i.a.), nas doses de 1,0, 1,5 e 2,0 l/ha, e a 240 g/l (i.a.), nas doses de 2,0, 3,0 e 4,0 l/ha. Como tratamento secundário (subparcelas) considerou-se o modo de aplicação do produto (pré ou pós-emergência das plantas daninhas) e como sub-subparcelas, as diferentes épocas de avaliação da eficácia de controle. As mudas foram plantadas no espaçamento de 0,5 x 0,5 m e os tratamentos foram aplicados por meio de um pulverizador costal pressurizado a CO2, a uma pressão de 2,45 kg/cm², utilizando-se um volume de calda igual a 200 l/ha. Os resultados mostraram que o herbicida oxyfluorfen formulado a 480 g/l e 240 g/l mostrou-se eficiente no controle de Brachiaria decumbens, Panicum maximum, Ipomoea grandifolia e Sida rhombifolia em diferentes épocas de avaliação, tanto quando foi aplicado em pré como em pós-emergência, sem ocasionar danos às plantas de Pinus caribea var. hondurensis.